US3137693A - Substituted pyrido [2, 3-e]-as-triazine 1-oxides - Google Patents

Substituted pyrido [2, 3-e]-as-triazine 1-oxides Download PDF

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Publication number
US3137693A
US3137693A US171807A US17180762A US3137693A US 3137693 A US3137693 A US 3137693A US 171807 A US171807 A US 171807A US 17180762 A US17180762 A US 17180762A US 3137693 A US3137693 A US 3137693A
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Prior art keywords
triazine
oxide
methylpyrido
formula
reaction
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Expired - Lifetime
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US171807A
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English (en)
Inventor
Carbon John Anthony
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Abbott Laboratories
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Abbott Laboratories
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Priority to US171807A priority Critical patent/US3137693A/en
Priority to GB4305/63A priority patent/GB1023218A/en
Priority to DEA42286A priority patent/DE1188605B/de
Priority to FR932768A priority patent/FR2498M/fr
Application granted granted Critical
Publication of US3137693A publication Critical patent/US3137693A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D471/00Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00
    • C07D471/02Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00 in which the condensed system contains two hetero rings
    • C07D471/04Ortho-condensed systems

Definitions

  • These compounds are crystalline solids useful as tranquilizers and antibacterial agents. When dispersed in water at a concentration of 50 parts per million, they inhibit the growth of bacteria such as Escherichia coli, Salmonella typhimurium and Staphylococcus aureas..
  • All of the compounds, other than Where Y is mercapto, can be prepared by the reaction of two molecular proportions of a compound of the formula H-Y with one molecular proportion of a compound of the formula in an inert solvent such as chloroform at a temperature of O0 C.
  • an inert solvent such as chloroform
  • the reaction mixture is poured into ice-water, the product extracted with chloroform, the solvent evaporated and the residue purified by recrystalilzation from an organic solvent such as ethanol or a mixture of ethanol and water.
  • the compounds wherein Y is mercapto are prepared by refluxing an alcoholic solution of two parts of thiourea and one part of a compound of the formula N @1 N N and thereafter separating the solid product formed followed by purification of said product by dissolution in aqueous alkali and reprecipitation with acetic acid.
  • Example 1 3 diethylamin0pyrido[2,3 e] as triazine 1 0xide.--One-tenth mole of 3-chloropyrido[2,3-e]-as-triazine l-oxide was dissolved in 300 ml. of chloroform and cooled to 0 C. A solution of 0.21 mole of diethylamine in 120 ml. of chloroform was then added portionwise while maintaining the temperature below 10 C. After standing at 5 C. for one hour, the reaction mixture was poured into ice-water, the solid product which formed Was extracted with chloroform and the chloroform evaporated. The residue was purified by recrystallization from ethanol to obtain the desired product which melted at 124-125 C.
  • Example 2 The reaction of 3-chloropyrido[2,3-e]-as-triazine l-oxide with piperidine in the same manner as that described in Example 1 produced 3-piperidinopyrido[2,3-e1-as-triazine l-oxide which melted at 116l17 C.
  • Example 3 By substituting morpholine for the diethylamine of Example 1, there is obtained 3-morpholinopyrido[2,3-e1- as-triazine l-oxide melting at 169170 C.
  • Example 4 The substitution of cyclohexylamine for diethylamine in Example 1 will produce 3-cyclohexylaminopyrido- [2,3-e1-as-triazine l-oxide which melts at -191 C.
  • Example 5 Replacing diethylamine of Example I with phenethylamine results in the production of 3-phenethylaminopyrido[2,3-e]-as-triazine l-oxide which has a melting point of 174-175 C.
  • Example 6 The reaction of n-butylamine with 3-chloropyrido- [2,3-e]-as-triazine l-oxide as described in Example 1 produces 3-n-butylaminopyrido[2,3-e1-as-triazine l-oxide melting at 174175 C.
  • Example 7 The replacement of diethylamine of Example 1 with dimethylaminopropylamine readily fortms 3-dimethylaminopropylaminopyrido[2,3-e1-as-triazine l-oxide which melts at 250-251 C. with decomposition.
  • Example 8 In the same manner as that described in Example 1, the reaction of hydrazine with 3-chloropyrido[2,3-e]-astriazine l-oxide will produce 3-hydrazinopyrido[2,3-e]- as-triazine l-oxide melting at 252-253 C. with decomposition.
  • Example 9 Reacting sodium methoxide or sodium n-butoxide with 3-chloropyrido[2,3-e]-as-triazine l-oxide as described in Example 1 will produce 3-methoxypyrido[2,3-e] -as-triazine l-oxide and 3-n-butoxypyrido[2,3-e]-as-triazine l-oxide, respectively, the former of which melts at 149 C. with decomposition and the latter of which melts at 99-l00 C.
  • Example 10 When 3-chloropyrido[2,3-e]-as-triazine l-oxide is reacted in the manner described in Example 1 with ethanol, isopropanol, dimethylamine, di-n-propylamine, methylamine, ethylamine, isopropylamine, diethylaminoethylamine, dipropylaminomethylamine or dimethylaminobutylamine there is obtained respectively, 3-ethoxypyrido[2,'3-e]-as-triazine l-oxide 3-isopropoxypyrido[2,3-e]-as-triazine 1-oxide 3-dimethylaminopyrido[2,3-e]-as-triazine l-oxide 3-di-n-propylaminopyrido [2,3-e] -as-triazine l-oxide -3-methylaminopyrido[2,3-e]
  • Example 13 By following the procedure of Example 1, the reaction of a compound of the formula N N wherein R is ethyl, propyl, butyl, chloro, bromo, fluoro or iodo with a monoloweralkylamine, diloweralkylamine, lower alkanol, hydrazine, piperidine, morpholine, cyclohexylamine, phenethylamine, or diloweralkylaminoloweralkylamine will produce compounds of the formula wherein R is as defined above and Y is methylamino, ethylamino, propylamino, butylamino, dimethylamino, diethylamino, dipropylamino, dibutylamino, Inethoxy,
  • the 3-chloro-7-R-pyrido[2,3-e]-as-triazine l-oxides employed as starting materials in the present invention can be prepared by refluxing two parts of guanidine and one part of a compound of the formula in a solvent such as t-butyl alcohol to form a compound of the formula which is heated on a steam bath with water in the presence of a catalyst such as potassium carbonate to obtain a compound of the formula A:NH2 N N which is thereafter reacted at about 20 C. with sodium nitrite in an acidified aqueous medium to obtain a con1- pound of the formula which is then refluxed with excess phosphorus oxychloride.
  • a solvent such as t-butyl alcohol
  • a catalyst such as potassium carbonate
  • a compound of the formula I ta wherein R is a member of the group consisting of hydrogen, lower alkyl and halogen and Y is a member of the group consisting of monoloweralkylamino, diloweralkylamino, loweralkoxy, hydrazino, piperidino, morpholino, cyclohexylamino, phenethylamino, mercapto and diloweralkylaminoloweralkylamino.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
  • Nitrogen Condensed Heterocyclic Rings (AREA)
US171807A 1962-02-08 1962-02-08 Substituted pyrido [2, 3-e]-as-triazine 1-oxides Expired - Lifetime US3137693A (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
US171807A US3137693A (en) 1962-02-08 1962-02-08 Substituted pyrido [2, 3-e]-as-triazine 1-oxides
GB4305/63A GB1023218A (en) 1962-02-08 1963-02-01 Substituted pyrido [2,3-e]-triazine 1-oxides
DEA42286A DE1188605B (de) 1962-02-08 1963-02-08 Verfahren zur Herstellung von Pyrido-[2, 3-e] [1, 2, 4]-triazin-1-oxyden
FR932768A FR2498M (fr) 1962-02-08 1963-04-26 Dérivés substitués d'oxyde-1 de pyrido (2,3-e)-triazine-as comme tranquillisants et agents antibactériens.

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US171807A US3137693A (en) 1962-02-08 1962-02-08 Substituted pyrido [2, 3-e]-as-triazine 1-oxides

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US3137693A true US3137693A (en) 1964-06-16

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DE (1) DE1188605B (fr)
FR (1) FR2498M (fr)
GB (1) GB1023218A (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3453276A (en) * 1966-10-06 1969-07-01 Smithkline Corp Triazinoindole compounds
US3549632A (en) * 1969-01-13 1970-12-22 American Cyanamid Co 3-aminopyrido(4,3-e)-as-triazine and 3 - aminopyrido(4,3-e)-as-triazine-1-oxide
US4324786A (en) * 1979-04-28 1982-04-13 Egyt Gyogyszervegyeszeti Gyar Pyrido[2,3-e]-as-triazine derivatives and pharmaceutical compositions

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2489355A (en) * 1947-01-10 1949-11-29 Merck & Co Inc Benzotriazines

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2489355A (en) * 1947-01-10 1949-11-29 Merck & Co Inc Benzotriazines

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3453276A (en) * 1966-10-06 1969-07-01 Smithkline Corp Triazinoindole compounds
US3549632A (en) * 1969-01-13 1970-12-22 American Cyanamid Co 3-aminopyrido(4,3-e)-as-triazine and 3 - aminopyrido(4,3-e)-as-triazine-1-oxide
US4324786A (en) * 1979-04-28 1982-04-13 Egyt Gyogyszervegyeszeti Gyar Pyrido[2,3-e]-as-triazine derivatives and pharmaceutical compositions

Also Published As

Publication number Publication date
FR2498M (fr) 1964-04-27
DE1188605B (de) 1965-03-11
GB1023218A (en) 1966-03-23

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